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INSTRUCTIONS FOR USE

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CAPP
Cloud and Pour Point
Refrigerator Bench -68C
ASTM D 97; ASTM D 2500; ASTM D 5853
IP 15; IP 219; DIN EN 23015

CFPP
Cold Filter Plugging Point
Refrigerator Bench -68C
ASTM D 6371; DIN EN 116; IP 309
SIS 155 122 (former DIN 51 428)

Quality Management System

The Petrotest GmbH Quality Management System:
Design, Manufacture, Sale and Repair of Petroleum Testing Devices
and Consistency Testing Devices according to the Requirements
DIN EN ISO 9001:2008. Certification Number 01 100 005115

Petrotest GmbH
A company of Anton Paar
Ludwig-Erhard-Ring 13
15827 Dahlewitz - Germany

Phone:
Fax:
E-Mail:
Website:

+49 (0)33708 56-300

+49 (0)33708 56-556
info@petrotest.com
www.petrotest.com

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TABLE OF CONTENTS
1. Important Notes ........................................................................................................................ 4
1.1. Liability ................................................................................................................................. 4
1.2. Warranty ............................................................................................................................... 4
1.3. Service ................................................................................................................................. 5
1.4. General Safety Information ................................................................................................... 5
1.5. Device-specific Safety Information ........................................................................................ 6
1.6. Summary of all Warnings in this Document .......................................................................... 6
2. Technical Specifications of the Device ................................................................................... 7
3. Device Parts .............................................................................................................................. 7
4. Bringing into Service ................................................................................................................ 8
4.1. Preselection of the cooling temperature at the controller ...................................................... 9
5. Scope CAPP ............................................................................................................................ 10
5.1. Accessories CAPP ............................................................................................................. 10
5.2. Spare Parts CAPP .............................................................................................................. 10
6. ASTM D 97 ............................................................................................................................... 11
6.1. Procedure ........................................................................................................................... 11
6.2. Calculation and Report ....................................................................................................... 13
6.3. Precision and Bias .............................................................................................................. 13
7. ASTM D 2500 ........................................................................................................................... 14
7.1. Procedure ........................................................................................................................... 14
7.2. Report ................................................................................................................................ 16
7.3. Precision and Bias .............................................................................................................. 16
8. Scope CFPP ............................................................................................................................ 17
8.1. Accessories CFPP.............................................................................................................. 17
8.2. Spare Parts CFPP .............................................................................................................. 18
9. ASTM D 6371 ........................................................................................................................... 18
9.1. Procedure ........................................................................................................................... 20
9.2. Precision and Bias .............................................................................................................. 22

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1. IMPORTANT NOTES
1.1. Liability
The device is an electrically operated appliance. It may not be operated unattended or in
areas at risk of explosion or damp locations. Whenever the device is used, a thorough
knowledge of the Instructions for Use and compliance with same is assumed. In all cases the
operator is liable for the safe operation of the device if it is not used according to instructions.
Repair of the device must be carried out only by Petrotest GmbH. Only original Petrotest
parts and replacement parts must be used to operate the device.
Petrotest is not responsible for damage or malfunctions caused by the operator using the
device improperly or contrary to the instructions. We reserve the right to make technical
changes.
Caution
This device is not to be used in explosive atmospheres!

1.2. Warranty
1. Petrotest products are warranted against defects in material and workmanship for a
period of one year from the date of purchase.
2. Petrotest will replace or repair products - free of any charge - that fail as a result of
defective materials or workmanship within the warranty period.
3. None of the obligations of Petrotest shall apply to any products which have been
subjected to misuse, neglect, accident or any extreme environmental condition or
improper handling.
4. If defective products are returned to Petrotest, the costs of such return will be borne by
the customer, and those of delivering the repaired or replacement products to the
customer will be borne by Petrotest.
Petrotests sole liability shall be to repair or replace any product which proves to be defective.
In no event shall Petrotest be liable for any special incidental, consequential, indirect or other
similar damages arising from failure of its products.

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1.3. Service
Should you require service, please contact our service department:
Petrotest GmbH
A company of Anton Paar
Ludwig-Erhard-Ring 13
15827 Dahlewitz - Germany

Phone:
+49 (0)33708 56-300
Fax:
+49 (0)33708 56-556
E-Mail:
service@petrotest.com
Website:
www.petrotest.com

1.4. General Safety Information

1. The device should only be used by trained personnel or those who have been instructed
accordingly.
2. Alterations on the device, especially opening of same or changes to the electrical
connections/electronic devices should only be done by company trained service
technicians and only after receiving permission from Petrotest GmbH.
3. Unauthorized changes will also cause refusing warranty issues by Petrotest.
4. Before opening the device, disconnect the electrical current.
5. If heating devices are used, please ensure that there are no combustible materials near
the heating source.
6. For safety reasons, we recommend using an earth leakage circuit breaker. Ask your
electrician for further details and equipment.
7. We make these recommendations on the assumption that a regular function and safety
test is performed at least every two years.
8. Do not dispose of the device in ordinary household waste! In light of the long lifespan of
the device, regulations may change. For this reason, please only delegate the disposal of
the device to qualified personnel or speak to Petrotest!
For EU countries:
Directive 2002/96/EC: Directive 2002/96 of the European Parliament and of
the Council of 27 January 2003 on waste electrical and electronic
equipment. (Petrotest Registration Number WEEE 80418806).
The directive describes the obligation to not dispose of electrical and
electronic devices as unsorted municipal waste and to collect this WEEE
separately. Contact us for an authorized waste disposal company in your
country.
The product described in these instructions conforms with:
EC Low-Voltage Directive 73/23/EEC and 93/68 EEC respectively.
EMC Directive 2004/108/EC.

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1.5. Device-specific Safety Information

The apparatus doesn't constitute a potential danger for the operators that use it or for what
operate in the zones surrounding; notwithstanding this, we beg to follow the indications
below.
1. Avoid leaning any kind of material on the apparatus.
2. Operators without qualification must not approach the operating
area.
3. Always wear suitable garments.

4. Always use masks, protective glasses and gloves conforming to

the normative in force.
5. Avoid sending water-spout on the device.
6. Always pay attention to use of the apparatus.
7. It is severely forbidden to smoke next to the apparatus.

1.6. Summary of all Warnings in this Document

1. When setting up the device select a location away from heat, smoke, electrical or
magnetic interference and avoid excessive electrostatic discharges (ESD) to the device.
The bench top must be a level surface and free of vibration.
2. The device is tested to comply with the limits of the European Electromagnetic
Compatibility (EMC) Directive 2004/108/EC. However this device generates radio
frequency energy. If the device is not installed or used in accordance with the instruction
manual it may cause interference to radio communications.
3. Ensure the heater of the device is not exposed to flammable liquids or other combustible
material including the packaging material. Clean the surface before starting a heater test.

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2. TECHNICAL SPECIFICATIONS OF THE DEVICE

Power supply:

230 Vac 10%, 50/60 Hz

Max. power consumption:

1300W

Motors:

1/3 hp gas R404A

5/8 hp gas R404A

Operating range:

ambient to -68C

Precision:

1C

Dimensions (W x D x H):

600 x 700 x 1000 mm

Weight:

120 Kg

Working temperature:

0 to 50C

Storage temperature:

-10 to 70C

Ambient relative humidity:

lower than 90% rH not condensing

3. DEVICE PARTS
Earth leakage
circuit breaker

Power switch

Heating switch

Temperature controller

Graphic 13-2418A

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4. BRINGING INTO SERVICE

Place the apparatus to at least 50 cm from possible obstacles which you wall up, other
apparatuses, etc., in such way that the air scoop has a good circulation of air.
The cooling cryostat consists of an aluminum block and an air-cooled chiller.
The cryostat is protected against too high voltage by an earth leakage circuit breaker.
For safety reasons the earth leakage circuit breaker must be switched manually once a
week for checking its correct function.
Please before connecting to the mains make sure the voltage corresponds to the value
on the device's rear side.
Before switching on the device the first time the power switch and the earth leakage circuit breaker
are set to 0.
Switch on earth leakage circuit breaker: "I".
Switch on power switch.

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4.1. Preselection of the cooling temperature at the controller

To modify the temperature of job (set point) on the digital thermo regulator hold arrow downkey. The display will show alternately the actual temperature and SP1. Now it is possible to
enter/modify set point value by pressing arrow-keys.
The value will be stored automatically after some seconds or press key P to confirm
immediately.
To this point follow the standard ASTM.
Press key HEATING to bring the apparatus to room temperature after a test.
It is not possible to control the heater by setting the temperature at temperature controller.
The device is always heated up to 25C.
This takes about 1h.
To re-cool the apparatus switch the heater off.
NOTE:
To heat the apparatus the main switch and heating switch must be in Position "I"!

Graphic 13-2418B

Earth leakage circuit breaker

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Power switch

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Heating switch

Temperature controller

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5. SCOPE CAPP
Standard test method for pour point for use on any petroleum products (ASTM D 97) and only
petroleum products which are transparent in layers 40 mm. in thickness and with a cloud point
below 49C.

5.1. Accessories CAPP

16-0361

Test jar ASTM standard

16-0363

Insulating disks

16-0367

Distance ring (set of 10 pcs.)

16-0371

Thermometer ASTM 5C

16-0375

Thermometer ASTM 6C

5.2. Spare Parts CAPP

Order of quantity

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16-0361

Test jar ASTM standard

10-0493

Insulating disks

10

16-0367

Distance ring, set of 10 pcs.

16-0371

Thermometer ASTM 5C

16-0375

Thermometer ASTM 6C

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6. ASTM D 97
6.1. Procedure
1. Pour the specimen into the test jar to the level mark. When necessary, heat the specimen
in a water bath until it is just sufficiently fluid to pour into the test jar.
NOTE
When the sample has been heated to a temperature higher than 45C during the
preceding 24 h or when the thermal history of the sample is not known, keep the sample
at room temperature for 24 h before testing it.
2. Close the test jar with the cork carrying the high-pour thermometer. See that the
thermometer and the jar are coaxial, and the thermometer bulb is immersed so the
beginning of the capillary is 3 mm below the surface of the specimen.
If the expected Pour point is above +36C use a higher range thermometer such as
IP63C or ASTM 61C.
Thermometer
High Cloud and Pour
Low Cloud and Pour
Melting Point

Temperature Range
-38 to +50C
-80 to +20C
+32 to +127C

Thermometer Number
ASTM
IP
5C
1C
6C
2C
61C
63C

3. For the measurement of pour point, subject the specimen in the test jar to the following
preliminary treatment:
1. Samples having Pour Points above -33C
Heat the specimen without stirring to 9C above the expected pour point, but to at
least 45C, in a bath maintained at 12C above the expected pour point, but at least
48C. Transfer the test jar to a water bath maintained at 24C and commences
observations for pour point.
2. Samples having Pour Points of -33C and below
Heat the specimen without stirring to 45C in a bath maintained at 48C and cool to
15C in a water bath maintained at 6C. Remove the high cloud and pour
thermometer and place the low cloud and pour thermometer in position.
4. Clean and dry the disk and the inside of the jacket to avoid frost formation which may
cause erroneous results.
Place the disk in the bottom of the jacket. Place the distance ring around the test jar
25mm from the bottom. Insert the test jar with distance ring in the jacket.

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5. Begin to examine the appearance of the specimen when the temperature of the
specimen is 9C above the expected pour point (estimated as a multiple of 3C). At each
test thermometer reading that is a multiple of 3C below the starting temperature remove
the test jar from the jacket and remove condensed moisture with a clean cloth moistened
in alcohol (ethanol or methanol).
Tilt the jar just enough to ascertain whether there is a movement of the specimen in the
test jar. The complete operation of removal, wiping, and replacement shall require not
more than 3 s.
Take great care not to disturb the mass of specimen nor permit the thermometer to shift
in the specimen; any disturbance of the spongy network of wax crystals will lead to low
and erroneous results.
If the specimen has not ceased to flow when its temperature has reached 27C, transfer
the test jar to the next lower temperature bath per the following schedule:
Bath
1
2
3
4
5

Bath temperature setting (C)

0 1,5
-18 1,5
-33 1,5
-51 1,5
-69 1,5

Sample temperature range (C)

Start to 9
9 to 6
-6 to 24
-24 to 42
-42 to -60
Table 1 Bath and sample temperature range

If the specimen in the jar does not flow when tilted, hold the jar in a horizontal position for
5 s and observe carefully. If the specimen shows any movement, replace the test jar
immediately in the jacket and repeat a test for flow at the next temperature, 3C lower.
6. If the specimen shows no movement when the test jar is held in a horizontal position for
5s. Record the observed reading of the test thermometer.
NOTE
To determine compliance with existing specifications having pour point limits at
temperatures not divisible by 3C, it is acceptable practice to conduct the pour point
measurement according to the following schedule: Begin to examine the appearance of
the specimen when the temperature of the specimen is 9C above the specification pour
point. Continue observations at 3C intervals as described in 6 and 7 until the
specification temperature is reached. Report the sample as passing or failing the
specification limit.
7. For black specimen, cylinder stock and non-distillate fuel specimen, the result obtained
by the procedure described in 1 through 6 is the upper (maximum) pour point. If required,
determine the lower (minimum) pour point by heating the sample while stirring, to 105C,
pouring it into the jar, and determining the pour point as described in 4 through 6.

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6.2. Calculation and Report

Add 3C to the temperature recorded in 7. and report the result as the Pour Point, ASTM D
97. For black oil, etc., add 3C to the temperature recorded in 7. and report the result as
Upper Pour Point, ASTM D 97, or Lower Pour Point, ASTM D 97, as required.

6.3. Precision and Bias

Lubricating Oil and Distillate and Residual Fuel Oil.
Repeatability
The difference between successive test results, obtained by the same operator using the
same apparatus under constant operating conditions on identical test material, would in the
long run, in the normal and correct operation of this test method, exceed 6C for Lubricating
Oils and 3C for middle Distillate and Residual Fuels only in one case in twenty. Differences
greater than this should be considered suspect.
Reproducibility
The difference between two single and independent test results, obtained by different
operators working in different laboratories on identical test material, would in the long run, in
normal and correct operation of this test method, exceed 9C for Lubricating Oil and Distillate
and Residual Fuels only in one case in twenty. Differences greater than this should be
considered suspect.
Bias
There being no criteria for measuring bias in these test-product combinations, no statement
of bias can be made.

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7. ASTM D 2500
7.1. Procedure
1. Bring the sample to a temperature at least 14C above the approximate cloud point.
Remove any moisture present by a method such as filtration through dry lintels filter
paper until the oil is perfectly clear, but make such filtration at a temperature of at least
14C above the approximate cloud point.
NOTE
In most cases of interference, filtration through dry lintels filter papers is sufficient. In the
case of diesel fuels, however, if the haze is very dense, a fresh portion of the sample
should be dried by shaking 100 mL with 5 g of anhydrous sodium sulphate for at least 5
min and then filtering through dry lintels filter paper. Given sufficient contact time, this
procedure will remove or sufficiently reduce the water haze so that the wax cloud can be
readily discerned. Drying and filtering should be done always at a temperature at least
14C above the approximate cloud point but otherwise not in excess of 49C
2. Pour the sample into the test jar to the level mark.
3. Close the test jar tightly with the cork carrying the thermometer.
The thermometer and the jar are coaxial, and the thermometer bulb is resting on the
bottom of the jar.
If the expected cloud point is above -36C use the High Cloud and Pour Point
Thermometer and the Low Cloud and Pour Point Thermometer if the expected cloud
point is below -36C.
Thermometer
High Cloud and Pour
Low Cloud and Pour

Temperature Range
-38 to +50C
-80 to +20C

Thermometer Number
ASTM
IP
5C
1C
6C
2C

NOTE
Thermometers should be checked immediately prior to the test and used only if their ice
points are 0 1C, when the thermometer is immersed to the immersion line in an ice
bath, and when the emergent column temperature does not differ significantly from 21C.
Alternatively, immerse the thermometer to a reading and correct for the resultant cooler
stem temperature.
4. To avoid frost formation which may cause erroneous results see that the disk, distance
ring, and the inside of the jacket are clean and dry.
Place the disk in the bottom of the jacket. The use of a jacket cover while the empty
jacket is cooling is permitted.
Place the distance ring around the test jar, 25 mm from the bottom. Insert the test jar in
the jacket.
5. Maintain the temperature of the cooling bath at 0 1.5C.

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6. At each test thermometer reading that is a multiple of 1C, remove the test jar from the
jacket quickly and without disturbing the oil, inspect for cloud, and replace in the jacket.
This operation shall require not more than 3 s. If the oil does not show a cloud when it
has been cooled to 9C, transfer the test jar to a second bath maintained at a
temperature of -18 1.5 C.
If the oil does not show a cloud when it has been cooled to
-6C, transfer the test jar to a third bath maintained at a temperature of
-33 1.5C. For the determination of very low cloud points additional baths are required,
each bath to be maintained in accordance with the following schedule.
Bath
1
2
3
4
5

Bath temperature setting (C)

0 1,5
-18 1,5
-33 1,5
-51 1,5
-69 1,5

Sample temperature range (C)

Start to 9
9 to 6
-6 to 24
-24 to 42
-42 to -60
Table 1 Bath and sample temperature range

7. Report the cloud point, to the nearest 1C, at which any cloud is observed at the bottom
of the test jar, which is confirmed by continued cooling.
NOTE
A wax cloud or haze is always noted first at the bottom of the test jar where the
temperature is lowest. A slight haze throughout the entire sample, which slowly becomes
more apparent as the temperature is lowered, is usually due to traces of water in the oil.
Generally this water haze will not interfere with the determination of the wax cloud point.
Dry the sample as described in 1.

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7.2. Report
Report the temperature recorded in 7 as the Cloud Point, Test Method D 2500.

7.3. Precision and Bias

The precision of this test method as determined by statistical examination of inter-laboratory
results is as follows:
Repeatability
The difference between two test results, obtained by the same operator with the same
apparatus under constant operating conditions on identical test material, would in the long
run, in the normal and correct operation of this test method exceed 2C only in one case in
twenty.
Reproducibility
The difference between two single and independent results obtained by different operators
working in different laboratories on identical test material, would in the long run, in the normal
and correct operation of this test method, exceed 4C for distillate Fuels and lubricating Oils
and 3C for Biodiesel Products only in one case in twenty.
Bias
The procedure in this test method has no bias, because the value of cloud point can be
defined only in terms of a test method.

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8. SCOPE CFPP
This test method covers for the determination of the cold filter plugging point temperature of diesel
and domestic heating fuels.

8.1. Accessories CFPP

13-0422

Test jar

13-0445

Air Jacket nickel-plated brass

13-0424

Glass pipette with 20ml level

13-0446

Holding ring

13-0428

Sleeve for thermometer

13-0447

Stopper made of plastic

16-0371

Thermometer ASTM 5C/IP 1C

13-0444

Centering rack

16-0375

Thermometer ASTM 6C/IP 2C

13-0430

Filter apparatus complete

Graphic 13-0421A

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8.2. Spare Parts CFPP

13-0422

test jar

13-0424

glass pipette with 20ml level

13-0427

filter socket with sieve

16-0371

thermometer ASTM 5C

13-0428

sleeve for thermometer

13-0414

grip with cylinder inset

9. ASTM D 6371

Graphics 13-0450C

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Prior to each test, the filtration unit in its individual parts, the test vessel, the pipette and the
thermometer must be washed with heptane.
Afterwards rinse with acetone and all parts are to be dried in a filtered airstream.
The cleaned and dried filtration unit is reassembled as shown in Illustration 13-0430A.

Fig. 13-0430A

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9.1. Procedure
1. A sample of 50 ml is filtered through a dry lint-free filter paper at room temperature
(>15C). Establish the cooling bath temperature at -34 0.5C
2. Place the centering rack in the jacket.
3. The filtered sample is filled into the test jar up to the mark.
The test jar is sealed with a stopper into which the glass pipette with the filtration unit and
the proper thermometer (see table) are inserted.
The lower edge of filtration unit must remain on the bottom of the test jar - see illustration
13-0421 A. The thermometer is not allowed to touch the wall of the test jar or the filtration
unit.
Expected CFPP
above -30 C
below -30C

Measuring range
-38C to +50C
-80C to +20C

Thermometer
ASTM
IP
5C
1C
6C
2C

Do not change thermometers during the test. Adjust the apparatus in such a way that the
bottom of the complete filter apparatus rests on the bottom of the test jar, and position the
thermometer so that its lower end is 1.5 0.2 mm above the bottom of the test jar.
NOTE
The position of the lower end of the thermometer above the bottom of the test jar can be
indirectly measured by marking the stem of the thermometer flush with the stopper when
the lower end of the thermometer is just touching the bottom of the test jar, and then
pulling the thermometer up such that the reference line is 1.5 0.2 mm above the top of
the stopper.
4. Insert the test jar assembly in a vertical position into the jacket.
5. With the stopcock open to atmosphere; connect the glas pipette to the vacuum system by
means of flexible tubing attached to the stopcock.
6. Switch on the vacuum unit.
The U-tube manometer must indicate a vacuum of 2001 mm.
7. Start the test immediately, but if the cloud point of the sample is known, it is permitted to
wait until the specimen has cooled to a temperature of not less than 5C above its cloud
point.
8. If the temperature of the sample has reached an suitable integer value, the three-way
cock is set to connect the filtration unit with the vacuum system, and the timer is switched
on.
This causes the sample to be drawn through the sieve of the filtration unit into the pipette.
If the sample has reached the mark on the pipette, the three-way cock assumes its
original position and the timer is stopped. Now the sample can flow back into the test jar
If the time required to reach the mark exceeds 60 s on the first attempt, the test
procedure is aborted and repeated with a new sample at a higher starting temperature.

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9. Test result
The measurement is repeated for each of the sample's 1C drop in temperature. If the
temperature has been reached at which the pipette is not filled up to the mark within 60 s,
the temperature at which the last filtration began is recorded as the CFPP. In case the
pipette has not been filled within 60 s, yet upon opening the pipette via the three-way
cock, the sample has not flowed back completely prior to the next intake cycle, the
temperature at the beginning of the last filtration is displayed as the CFPP.
10. In case the CFPP has not yet been reached when the sample temperature is -20C, the
test is to be continued in a second cooling bath in which the temperature is kept at a
constant -511C.
For this the test jar with the filter unit is quickly transferred into a air jacket which is in the
second cooling bath.
11. In case the CFPP has not been reached yet when the sample temperature is -35C, the
test is to be continued in a third cooling bath in which the temperature is kept at a
constant -672C.
12. In case no plugging of the filter occurs when the sample temperature is -51C, the
procedure is aborted. The result is recorded as "Not plugged at -51C".

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9.2. Precision and Bias

The precision of this procedure as determined by the statistical examination of the
interlaboratory test results is as follows:
Repeatability
The difference between results obtained on the same day by the same operator with the
same apparatus under constant operating conditions on identical test material, would in the
long run, with normal and correct operation of the test method, exceed 1.76C only in one
case in twenty.
Reproducibility
The difference between two single and independent results obtained by different operators
working in different laboratories on identical test material, would in the long run, in the normal
and correct operation of the test method, exceed the values indicated by the formula:
0.102 (25-X) C
Where:
X is the average of the two results being compared, only in one case in twenty.
Bias
The procedure in this test method has no bias because the value of CFPP can be defined
only in terms of a test method.
Relative Bias
The current inter-laboratory tests confirm that there is no relative bias between the manual
and automated apparatuses. Both apparatuses are suitable for reference purposes.

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